CN109748283A - A kind of hollow SiO of lithium ion batteryx@C cube composite negative pole material and preparation method - Google Patents
A kind of hollow SiO of lithium ion batteryx@C cube composite negative pole material and preparation method Download PDFInfo
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- CN109748283A CN109748283A CN201910171469.4A CN201910171469A CN109748283A CN 109748283 A CN109748283 A CN 109748283A CN 201910171469 A CN201910171469 A CN 201910171469A CN 109748283 A CN109748283 A CN 109748283A
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention provides a kind of lithium ion batteries with hollow SiOx@C cube composite negative pole material and preparation method, belong to technical field of lithium ion battery negative.The hollow SiOx@C cube composite negative pole material is followed successively by cavity, SiO from inside to outsidexWith three layers of carbon shell.Specific preparation process is as follows: using nanometer calcium carbonate as template, silica is grown in template, then one layer of organic carbon source is coated with liquid phase method again, passes through pyrolysis, carbon thermal reduction, pickling, the hollow SiO for being dried to obtain hypoxemia valuex@C nano cube composite negative pole material.The cube hollow structure of the composite negative pole material is SiOxVolume expansion provide space, so that material is kept stable structure during removal lithium embedded, the carbon of external sheath improves the electric conductivity of material, and then the comprehensive cycle life for promoting material.
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular to a kind of hollow SiO of lithium ion batteryx@C cube is multiple
Close negative electrode material and preparation method.
Background technique
With the fast development of new-energy automobile industry, have as the lithium ion battery of core component and power producer wide
The wealthy market space.Lithium ion battery is high with energy density, have extended cycle life, self discharge is few, charging rate is fast and environment is friendly
The advantages that good is the best secondary cell of current market prospects with fastest developing speed." made in China 2025 " proposes the year two thousand twenty monomer electricity
Pond energy density reaches 300Wh/kg.Realize above-mentioned target, there is an urgent need to develop lithium ion battery with high energy densities out.Mesh
Before, the graphite cathode theoretical capacity that lithium ion battery generallys use is only 372mAh/g, and actual capacity is difficult already close to the limit
It is improved again, it is difficult to meet the needs of electric car is higher and higher to battery energy density.
The theoretical capacity of silicon at normal temperature is 3580mAh/g, is ten times of graphite capacity or so.But silicon is in charge and discharge
Volume change in journey is up to 300%, easily causes active material dusting, falls off, and final the quick of conductive tankage declines
Subtract, further limits its commercial applications.The theoretical capacity of SiO is greater than 2000mAh/g, and the volume in charge and discharge process is swollen
Swollen only 200%, have more Commercial Prospect.Therefore the SiO based composites that development cycle is had excellent performance become this field skill
Art personnel focus of interest.
Summary of the invention
The purpose of the present invention is to provide a kind of hollow SiO of lithium ion batteryxThe preparation of@C cube composite negative pole material
Method, the hollow SiO of this method preparationx@C cube composite negative pole material has high specific capacity and excellent cycle performance.
A kind of hollow SiO of lithium ion batteryx@C cube composite negative pole material, it is characterised in that: the SiOx@C is compound
Negative electrode material is three-decker, is followed successively by cavity, SiO from inside to outsidexWith carbon shell；It is described hollow for nano cubic shape；It is described
SiOx@C composite negative pole material shape is nano cubic structure.
The SiOxThe granularity of@C composite negative pole material is 50~500nm.
A kind of hollow SiO of lithium ion battery as described abovexThe preparation method of@C cube composite negative pole material, it is described hollow
Shape SiOx@C negative electrode material is by SiOxIt is formed with two kinds of Material claddings of carbon, the SiOxGranularity be 30~200nm hollow nanometer
Cube, the carbon coating is in hollow nano cubic shape SiOxOn.Specifically preparation step includes:
(1) CaCO is prepared3@SiO2Nanocube: nanometer calcium carbonate is dispersed in the mixing of the ethyl alcohol and water of certain volume ratio
In solution, appropriate ammonium hydroxide is added, is stirred evenly, nano calcium carbonate suspension is obtained；Above-mentioned receive is added in tetraethyl orthosilicate
In rice calcium carbonate suspension, 7~12h is stirred at 25 DEG C~85 DEG C, centrifugation washing obtains silicon dioxide coated nano calcium carbonate
The composite material of cube, i.e. CaCO3@SiO2；
(2) CaCO is prepared3@SiOx@C-material: by organic carbon source, CaCO3@SiO2It being added in solvent, ultrasonic disperse is uniform,
It continues stirring until solvent evaporation completely, obtains the CaCO of organic carbon source cladding3@SiO2；The CaCO of organic carbon source cladding3@SiO2It sets
In tube furnace, be warming up to 500~900 DEG C, 2~5h of constant temperature with certain heating rate, be cooled to room temperature remember it is carbon-coated
CaCO3@SiOx, i.e. CaCO3@SiOx@C；
(3) hollow Void@SiOx@C nano cubic materials are prepared: by CaCO3@SiOx@C nano cubic materials are added
In certain density acid solution, stirring and pickling certain time removes the CaCO of innermost layer3, then clear with water and ethyl alcohol centrifugation
It washes 3~5 times, high temperature drying obtains Void SiOx C.
Further, 40~300nm of the granularity of the nanometer calcium carbonate in the step (1), the certain volume ratio
For ethyl alcohol: water=3~6:1, the appropriate ammonium hydroxide are the 1%~5% of ethyl alcohol and water mixed solution volume, the positive silicic acid tetrem
Ester is the 0.5%~2% of ethyl alcohol and water mixed solution volume.
Further, the organic carbon source in the step (2) is polyvinylpyrrolidone, glucose, pitch, the solvent
For water, ethyl alcohol, tetrahydrofuran, n-hexane.
Further, the acid solution in the step (3) is hydrochloric acid, and acetic acid, the concentration is 1M~5M, the pickling
Certain time is 2~10h, and the high temperature drying is 80 DEG C~300 DEG C dryings.
Preparation principle of the invention: using nanometer calcium carbonate as template, silica is grown in template, then uses liquid phase again
Method coats one layer of organic carbon source, obtains CaCO by pyrolysis, carbon thermal reduction3@SiOx@C, last pickling are dried to obtain hypoxemia value
Hollow SiOx@C nano cube composite negative pole material.
The present invention has the advantage that
(a) present invention is template using nanometer calcium carbonate, it is only necessary to can be removed, not needed with conventional hydrochloric acid, acetic acid
Template is removed using the hydrofluoric acid of severe toxicity, environmental pollution is small, and method is simple and safe, is suitble to large-scale production；
(b) present invention prepares hollow SiOx@C nano cubic materials, SiOxVolume expansion is small compared to the expansion of Si, more
Have using cyclical stability, while hollow structure is also SiOxVolume expansion leaves space, guarantees that nanocube structure is steady
It is fixed not rupture；
(c) SiO of the inventionxThe C cubic materials outer surface@has carbon coating layer, the electric conductivity of material can be improved, together
When avoid hollow SiOxNanocube particle is directly exposed in electrolyte, helps to improve coulombic efficiency for the first time.
Detailed description of the invention
Fig. 1 is the XRD spectrum of hollow SiOx@C cube negative electrode material prepared by the embodiment of the present invention 1.
Fig. 2 is the SEM photograph of hollow SiOx@C cube negative electrode material prepared by the embodiment of the present invention 1.
Fig. 3 is the Raman photo of hollow SiOx@C cube negative electrode material prepared by the embodiment of the present invention 2.
Fig. 4 is the TEM photo of hollow SiOx@C cube negative electrode material prepared by the embodiment of the present invention 2.
Fig. 5 is the SEM photograph of hollow SiOx@C cube negative electrode material prepared by the embodiment of the present invention 3.
Fig. 6 is the charging and discharging curve of hollow SiOx@C cube negative electrode material prepared by the embodiment of the present invention 3.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with attached drawing and specific implementation
Mode, the present invention will be described in further detail.Obviously, described embodiment is only that a part of the invention is implemented
Example, instead of all the embodiments.Based on the embodiments of the present invention, those skilled in the art is not making creative labor
Every other embodiment obtained under the premise of dynamic, shall fall within the protection scope of the present invention.It should be appreciated that tool described herein
Body embodiment only to explain the present invention, is not intended to limit the present invention.
Embodiment one
(1) CaCO is prepared3@SiO2Nanocube: 300mg nanometer calcium carbonate is dispersed in the mixing of the ethyl alcohol and water of 300mL
Solution (ethyl alcohol and water volume ratio=3:1), adds 3mL ammonium hydroxide, stirs evenly, obtain nano calcium carbonate suspension；Just by 2mL
Tetraethyl orthosilicate is added in above-mentioned nano calcium carbonate suspension, and 7h is stirred at 40 DEG C, and centrifugation washing obtains coated with silica
The composite material of nanometer calcium carbonate cube, i.e. CaCO3@SiO2；
(2) CaCO is prepared3@SiOx@C-material: by polyvinylpyrrolidone, CaCO3@SiO2It is added to the water, ultrasonic disperse is equal
It is even, it continues stirring until solvent evaporation completely, obtains the CaCO of polyvinylpyrrolidone cladding3@SiO2；Polyvinylpyrrolidone packet
The CaCO covered3@SiO2It is placed in tube furnace, is warming up to 600 DEG C with certain heating rate, constant temperature 2h is cooled to room temperature and remembers carbon
The CaCO of cladding3@SiOx, i.e. CaCO3@SiOx@C；
(3) hollow Void@SiOx@C nano cubic materials are prepared: by CaCO3@SiOx@C nano cubic materials are added
In the hydrochloric acid solution of 1M, stirring and pickling 4h removes the CaCO of innermost layer3, then use water and ethyl alcohol eccentric cleaning 3~5 times, 80 DEG C
Drying to obtain Void@SiOx@C.
The present invention has no special requirement and limitation to the rate of the heating, using liter well known to those skilled in the art
Warm rate.
Embodiment two
(1) CaCO is prepared3@SiO2Nanocube: 200mg nanometer calcium carbonate is dispersed in the mixing of the ethyl alcohol and water of 300mL
Solution (ethyl alcohol and water volume ratio=4:1), adds 6mL ammonium hydroxide, stirs evenly, obtain nano calcium carbonate suspension；Just by 3mL
Tetraethyl orthosilicate is added in above-mentioned nano calcium carbonate suspension, and 8h is stirred at 60 DEG C, and centrifugation washing obtains coated with silica
The composite material of nanometer calcium carbonate cube, i.e. CaCO3@SiO2；
(2) CaCO is prepared3@SiOx@C-material: by pitch, CaCO3@SiO2It being added in tetrahydrofuran, ultrasonic disperse is uniform,
It continues stirring until solvent evaporation completely, obtains the CaCO of pitch-coating3@SiO2；The CaCO of pitch-coating3@SiO2It is placed in tube furnace
In, 700 DEG C are warming up to certain heating rate, constant temperature 3h is cooled to room temperature and remembers carbon-coated CaCO3@SiOx, i.e.,
CaCO3@SiOx@C；
(3) hollow Void@SiOx@C nano cubic materials are prepared: by CaCO3@SiOx@C nano cubic materials are added
In the acetum of 5M, stirring and pickling 6h removes the CaCO of innermost layer3, then use water and ethyl alcohol eccentric cleaning 3~5 times, 120
DEG C drying to obtain Void@SiOx@C.
The present invention has no special requirement and limitation to the rate of the heating, using liter well known to those skilled in the art
Warm rate.
Embodiment three
(1) CaCO is prepared3@SiO2Nanocube: 400mg nanometer calcium carbonate is dispersed in the mixing of the ethyl alcohol and water of 300mL
Solution (ethyl alcohol and water volume ratio=6:1), adds 15mL ammonium hydroxide, stirs evenly, obtain nano calcium carbonate suspension；By 5mL
Tetraethyl orthosilicate is added in above-mentioned nano calcium carbonate suspension, and 10h is stirred at 80 DEG C, and centrifugation washing obtains silica packet
Cover the composite material of nanometer calcium carbonate cube, i.e. CaCO3@SiO2；
(2) CaCO is prepared3@SiOx@C-material: by glucose, CaCO3@SiO2It is added to the water, ultrasonic disperse is uniform, continues
Stirring completely, obtains the CaCO of glucose cladding to solvent evaporation3@SiO2；The CaCO of glucose cladding3@SiO2It is placed in tube furnace
In, 900 DEG C are warming up to certain heating rate, constant temperature 5h is cooled to room temperature and remembers carbon-coated CaCO3@SiOx, i.e.,
CaCO3@SiOx@C；
(3) hollow Void@SiOx@C nano cubic materials are prepared: by CaCO3@SiOx@C nano cubic materials are added
In the hydrochloric acid solution of 3M, stirring and pickling 10h removes the CaCO of innermost layer3, then use water and ethyl alcohol eccentric cleaning 3~5 times, 300
DEG C drying to obtain Void@SiOx@C.
SEM test is carried out to obtained composite negative pole material, as a result as shown in Figure 5.From fig. 5, it is seen that SiOx@C
In cube shaped frame, granularity is between 50~100nm.
By hollow shape SiOx@C composite negative pole material made from embodiment and conductive agent Super P and binder 70:15:15
Ground and mixed is carried out, slurry is prepared into, is then coated uniformly on copper foil with scraper, and dry 10h at 80 DEG C in vacuum tank, it
After carry out punching, with lithium metal be to electrode assembling button cell.Fig. 6 is that the charge and discharge in the case where current density is 500mA/g are bent
Line, after the circulation of 500 circles, specific capacity 663mAh/g has shown excellent cycle performance.
Claims (6)
1. a kind of hollow SiO of lithium ion batteryx@C cube composite negative pole material, it is characterised in that: the SiOx@C Compound Negative
Pole material is three-decker, is followed successively by cavity, SiO from inside to outsidexWith carbon shell；It is described hollow for nano cubic shape；The SiOx@C
Composite negative pole material shape is nano cubic structure.
2. hollow SiO according to claim 1x@C cube composite negative pole material, it is characterised in that the SiOx@C is multiple
The granularity for closing negative electrode material is 50~500nm.
3. a kind of hollow SiO of lithium ion batteryxThe preparation method of@C cube composite negative pole material, it is characterised in that: specific packet
Include following preparation step:
(1) CaCO is prepared3@SiO2Nanocube: nanometer calcium carbonate is dispersed in the ethyl alcohol of certain volume ratio and the mixed solution of water
In, appropriate ammonium hydroxide is added, is stirred evenly, nano calcium carbonate suspension is obtained；Above-mentioned nano-sized carbon is added in tetraethyl orthosilicate
In sour calcium suspension, 7~12h is stirred at 25 DEG C~85 DEG C, centrifugation washing obtains silicon dioxide coated nano calcium carbonate cube
The composite material of body, i.e. CaCO3@SiO2；
(2) CaCO is prepared3@SiOx@C-material: by organic carbon source, CaCO3@SiO2It is added in solvent, ultrasonic disperse is uniform, continues
Stirring completely, obtains the CaCO of organic carbon source cladding to solvent evaporation3@SiO2；The CaCO of organic carbon source cladding3@SiO2It is placed in pipe
In formula furnace, be warming up to 500~900 DEG C, 2~5h of constant temperature with certain heating rate, be cooled to room temperature remember it is carbon-coated
CaCO3@SiOx, i.e. CaCO3@SiOx@C；
(3) hollow Void@SiOx@C nano cubic materials are prepared: by CaCO3@SiOx@C nano cubic materials are added certain
In the acid solution of concentration, stirring and pickling certain time removes the CaCO of innermost layer3, then with water and ethyl alcohol eccentric cleaning 3~
5 times, high temperature drying obtains Void SiOx C.
4. the hollow SiO of a kind of lithium ion battery according to claim 3xThe preparation side of@C cube composite negative pole material
Method, it is characterised in that 40~300nm of the granularity of the nanometer calcium carbonate in the step (1), the certain volume ratio are second
Alcohol: water=3~6:1, the appropriate ammonium hydroxide are the 1%~5% of ethyl alcohol and water mixed solution volume, and the tetraethyl orthosilicate is
The 0.5%~2% of ethyl alcohol and water mixed solution volume.
5. the hollow SiO of a kind of lithium ion battery according to claim 3xThe preparation side of@C cube composite negative pole material
Method, it is characterised in that the organic carbon source in the step (2) is polyvinylpyrrolidone, glucose, pitch, and the solvent is
Water, ethyl alcohol, tetrahydrofuran, n-hexane.
6. the hollow SiO of a kind of lithium ion battery according to claim 3xThe preparation side of@C cube composite negative pole material
Method, it is characterised in that the acid solution in the step (3) is hydrochloric acid, and acetic acid, the concentration is 1M~5M, and the pickling is certain
Time is 2~10h, and the high temperature drying is 80 DEG C~300 DEG C dryings.
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Cited By (3)
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| CN111987298A (en) * | 2020-08-28 | 2020-11-24 | 成都新柯力化工科技有限公司 | Method for compounding lithium battery silicon carbon by using homogenizer and lithium battery silicon carbon cathode |
| CN113611864A (en) * | 2021-07-30 | 2021-11-05 | 江苏泛亚微透科技股份有限公司 | Carbon aerogel coated silica hollow microsphere negative electrode material |
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Application publication date: 20190514 |